Potassium Carbonate → alpha-Ethyl-alpha-(4-chlorophenyl)-4-[3-(di-n-propylamino)-propoxy]-benzylalcohol

HRID 236568

반응식

HRID 236568 반응식
[CH2:1]([C:3]([OH:18])([C:11]1[CH:16]=[CH:15][C:14]([Cl:17])=[CH:13][CH:12]=1)[C:4]1[CH:9]=[CH:8][C:7]([OH:10])=[CH:6][CH:5]=1)[CH3:2].C(=O)([O-])[O-].[K+].[K+].[CH2:25]([N:28]([CH2:32][CH2:33][CH2:34]Cl)[CH2:29][CH2:30][CH3:31])[CH2:26][CH3:27]>S([O-])(O)(=O)=O.C([N+](CCCC)(CCCC)CCCC)CCC.C(OCC)(=O)C>[CH2:1]([C:3]([OH:18])([C:11]1[CH:16]=[CH:15][C:14]([Cl:17])=[CH:13][CH:12]=1)[C:4]1[CH:5]=[CH:6][C:7]([O:10][CH2:27][CH2:26][CH2:25][N:28]([CH2:32][CH2:33][CH3:34])[CH2:29][CH2:30][CH3:31])=[CH:8][CH:9]=1)[CH3:2]

참가 물질

6

반응물 3

HCID 11430Potassium CarbonateHCID 12333917Dipropylaminopropyl chlorideHCID 14727318alpha-Ethyl-alpha-(4-chlorophenyl)-4-hydroxy-benzylalcohol

생성물 1

HCID 20216260alpha-Ethyl-alpha-(4-chlorophenyl)-4-[3-(di-n-propylamino)-propoxy]-benzylalcohol

시약·촉매·용매 2

HCID 94433Tetrabutylammonium hydrogen sulfate촉매HCID 8857Ethyl Acetate용매

실험 절차

13.1 g. of α-ethyl-α-(4-chlorophenyl)-4-hydroxy-benzylalcohol, 14 g. of anhydrous potassium carbonate, 9.8 g. of dipropylaminopropyl chloride and 0.85 g. of tetrabutyl ammonium hydrogensulfate in 135 ml. of ethyl acetate are slightly boiled for 20 hours, under stirring. After cooling the mixture, the solvent is evaporated in vacuo. To the residue water and benzene are added. The phases are separated, the benzene solution is washed with water, dried over anhydrous potassium carbonate, filtered and evaporated. The residue is purified by vacuum fractionation. 13.8 g. of the desired end product are obtained, boiling at 198° to 200° C./1.33 Pa.

후처리

  1. temperatureAfter cooling the mixture
  2. customthe solvent is evaporated in vacuo
  3. additionTo the residue water and benzene are added
  4. customThe phases are separated
  5. washthe benzene solution is washed with water
  6. dry with materialdried over anhydrous potassium carbonate
  7. filtrationfiltered
  8. customevaporated
  9. customThe residue is purified by vacuum fractionation
  10. customof the desired end product are obtained

출처 및 근거

ORD 기록
ord-207e32b5a3714d40af02fe0ad4959c98
출처 데이터셋
uspto-grants-1987_02
특허 번호
US04645779

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